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A kind of preparation method of vasopressin [4-glu]

A vasopressin and chromatography technology, applied in the field of preparation of vasopressin [4-Glu], can solve the problems of dilute sample concentration, low yield, complicated preparation process, etc., and achieve the effect of optimizing the production process

Active Publication Date: 2020-02-18
SPH NO 1 BIOCHEM & PHARMA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The technical problem to be solved by the present invention is to provide a kind of vasopressin [4-Glu] in order to overcome the defects of complex preparation process, low yield, dilute sample concentration and bulky volume in the prior art. -Glu] preparation method

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Example 1 (HPLC method to detect the crude product of vasopressin [4-Glu] precursor and the purity of the purified product solution)

[0031] Instrument: Waters 2695 / 2489 high performance liquid chromatography

[0032] Separation column: Agilent XDB-C18 4.6×250mm, 5μm

[0033] Mobile phase: A is 0.1% TFA aqueous solution in volume percentage, B is 0.1% TFA-50% acetonitrile aqueous solution in volume percentage (TFA is trifluoroacetic acid)

[0034] The flow rate is 1.0mL / min, the detection wavelength is 214nm, and it is detected at room temperature. The elution gradient is shown in the table below, and the percentages are volume percentages.

[0035] Elution step Elution time eluent 1 0~5min 95%A+5%B 2 5~25min 95%A+5%B→50%A+50%B 3 25~30min 100％B 4 30~35min 95%A+5%B

Embodiment 2

[0036] Embodiment 2 (75mm inner diameter L&L4003 preparative column packing)

[0037] Using Load&Lock dynamic axial compression and static locking technology, the filler is styrene-divinylbenzene copolymer (reversed phase packing Agilent PLRP-S), the pore size is 10nm, the particle size is 10μm, and the column packing density is 0.33g / mL. Bed pressure 650psi, using Varian chromatography packing system, 370g dry powder filler, 2L methanol after stirring and homogenizing, poured into the L&L4003 preparative column with an inner diameter of 75mm, the compression ratio is 3:1, and the carrier gas is N 2 , adjust the carrier gas pressure so that the pressure of the oil pressure gauge is 2000psi, and the dynamic axial compression reaches a column bed height of 26cm.

Embodiment 3

[0038] Example 3 Reverse-phase cyclization, reverse-phase purification and reverse-phase desalting of crude precursor material of vasopressin [4-Glu]

[0039] Instrument: Varian SD-1 high pressure liquid phase preparation system

[0040] Chromatographic column: self-packed preparative column Load&Lock4003 75×260mm in Example 2, PLRP-S 10μm 10nm

[0041] The crude product of vasopressin [4-Glu] precursor is the crude product of vasopressin [4-Glu] precursor obtained by cracking and drying by solid-phase synthesis method, and its structural formula is Cys-Tyr-Phe-Glu-Asn-Cys-Pro -Arg-Gly-NH 2 of trifluoroacetate.

[0042] The crude vasopressin [4-Glu] precursor solution is a 5 g / L solution formed by dissolving the above crude vasopressin [4-Glu] precursor in 5% acetonitrile aqueous solution.

[0043] Mobile phase A1 is purified water, A2 is 0.02 volume percent H 2 o 2 pH is the NaOH aqueous solution of 7.5, mobile phase B is acetonitrile, and mobile phase C1 is described vaso...

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Abstract

The invention discloses a preparation method for vasopressin[4-Glu]. The preparation method comprises the following step: successively subjecting a solution of a crude vasopressin[4-Glu] precursor product to reversed-phase cyclization, reversed-phase purification and reversed-phase desalination by adopting a highly-efficient liquid-phase reversed-phase chromatography process, wherein a filling material for the highly-efficient liquid-phase reversed-phase chromatography process is a styrene-divinyl benzene copolymer; and the crude vasopressin[4-Glu] precursor product contains two free sulfhydryl groups. The preparation method provided by the invention innovatively adopts a reversed-phase adsorption method for cyclization, purification and desalination, solves the problems of cyclization, purification and desalination once for all, optimizes production process, and is applicable to continuous industrial production.

Description

technical field [0001] The invention relates to the field of biopharmaceuticals. More specifically, the present invention relates to a preparation method of vasopressin [4-Glu]. Background technique [0002] Vasopressin is a synthetic polypeptide consisting of nine amino acid residues with a chemical structure of The theoretical molecular weight of vasopressin is 1084.24. Vasopressin tannin is an antidiuretic hormone drug, which can promote the reabsorption of water in the distal renal tubule and collecting duct and has an antidiuretic effect. Its preparation is clinically used for the treatment of diabetes insipidus. [0003] At present, most domestic vasopressin [4-Glu] first adopts solid-phase synthesis to protect vasopressin [4-Glu] resin, and then undergoes cracking and drying to obtain the crude product of vasopressin [4-Glu] precursor (Cys-Tyr-Phe- Glu-Asn-Cys-Pro-Arg-Gly-NH 2 Trifluoroacetic acid salt), highly diluted cyclization, purification, salt conversion a...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07K7/16C07K1/20
CPCC07K7/16
Inventor 江锡铭丁金国黄臻辉
Owner SPH NO 1 BIOCHEM & PHARMA CO LTD
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